CN109167064B - Composite binder applied to lithium ion battery anode material and preparation method thereof - Google Patents
Composite binder applied to lithium ion battery anode material and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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Abstract
The invention discloses a composite binder applied to a lithium ion battery anode material and a preparation method thereof, wherein an ionic polymer is dissolved in a solvent, a dispersion liquid of an electronic conductive polymer is added, and the mixture is mixed and then added with an adhesive for blending to obtain the composite binder. The invention also discloses a preparation step of the composite binder, which comprises (1) preparation of ionic polymer; (2) preparing a binder solution; (3) and (3) preparing a composite film. The composite binder prepared by the invention can be dissolved by a hydrosolvent or a non-hydrosolvent, so that the pollution problem to the environment is reduced, and the requirement of industrial production is met. Meanwhile, the composite binder has ionic conductivity and electronic conductivity, and an ionic/electronic conductive network is formed while the physical properties of the pole piece are met, so that the electrochemical performance of the battery is enhanced.
Description
Technical Field
The invention relates to the field of material chemistry and new energy, in particular to a composition and a preparation method of a composite binder and application of the composite binder prepared by the method to preparation of a lithium ion battery positive plate.
Background
The lithium ion battery is a representative of modern high-performance batteries, the production environment and the electrical performance of the lithium ion battery electrode depend on the preparation process of electrode slurry and electrode materials, and the good pulping process can improve the quality and the performance of products on one hand and can reduce the cost of raw materials and the time cost in the production process on the other hand. The binder, which is a constituent of the battery slurry, is uniformly dispersed in the solvent with the electrode active material, the conductive agent, and the like in a stirring manner, and although the amount used is low, the selection thereof is important. The lithium-storing active material will produce volume change continuously during the charging and discharging process of the battery, resulting in cracking and pulverization of the active material, and the conductive agent and the active material lose electric contact, thereby causing damage of the electrode structure and causing poor cycling stability and rate capability. Therefore, the binder needs to have sufficient flexibility to relieve the volume change of the electrode plate caused in the charging and discharging process, and increase the adhesion between the slurry and the current collector, so that the active substances do not fall off in the charging and discharging process, and the bonding state between the particles is not damaged. For lithium battery electrodes, the binder has high electron conductivity and tensile properties, and lithium ion diffusion and transport properties have a great influence on lithium storage properties.
In the current industrialized production process of the lithium ion battery anode, an oil lithium ion battery stirring system is adopted, a solvent type binder is used, an organic solvent NMP is adopted as a dispersing agent, such as polyvinylidene fluoride (PVDF), although the electrochemical performance of the PVDF is stable, the PVDF does not have ionic conductivity and electronic conductivity, so that the internal resistance and the electrochemical performance of the lithium ion battery are influenced; in addition, PVDF is too dependent on a single type of solvent, NMP is very easy to absorb water, and the later performance of the lithium ion battery is affected after water absorption, so that the environmental humidity must be strictly controlled in the manufacturing of the battery core, and the production and manufacturing cost is increased.
In order to solve the problems of selectivity of the solvent and electron ion insulation of the binder, researchers have begun to search for an aqueous composite conductive binder having both ion conductivity and electron conductivity.
The related inventions of the currently applied patent mainly include: (1) ion conductive type binder: patent document (CN102382321A) discloses that an ion-conductive polymer having hydrophobic and hydrophilic properties is used as a binder, and the solvent is a mixed bi-solvent of a strongly polar solvent and a weakly polar solvent. However, the method has poor electronic conductivity, complex material selection and poor heat resistance and solvent resistance, so that the performance of the battery is influenced to a certain extent. Another patent document (CN106299377A) discloses that a lithium salt branched polymer is used as a conductive binder, and Li + in the binder can be rapidly conducted at low temperature, thereby improving low temperature performance. Such binders have certain temperature-limiting requirements, for example, under high-temperature cycling, the Li + activity suffers certain loss, and the material structure also deteriorates, resulting in the high-temperature cycling capacity of the battery being degraded.
(2) Electron conductive binder: patent document (CN104282912A) discloses a binder in which polyvinylidene fluoride (PVDF) and a conductive polymer are compounded to form a conductive polymer crosslinked structure. The conductive polymer particles and the PVDF powder are blended in an N, N-dimethylformamide solvent, and the binder is prepared through a series of drying and ball milling processes. The conductive particles are not uniformly dispersed, a better conductive network cannot be formed, and polymer agglomeration caused by overhigh temperature is easy to generate, so that the electrode material is not beneficial to subsequent processing. Patent document (CN105047935B) discloses a conductive adhesive prepared by in-situ composite reaction of a conductive polymer monomer and an aqueous adhesive in the presence of an acidic medium. The conditions of the acidic medium required for this invention are not environmentally friendly and are therefore not suitable for industrial production.
(3) Conductive composite binder: the patent (CN105633411A) proposes that a certain amount of styrene-butadiene rubber is added into fully or partially neutralized lithium polyacrylate to form an aqueous composite binder with electron ion conductivity, so as to enhance the strength between the binder and a current collector, and the component lithium polyacrylate can also enhance the conductivity of lithium ions and electrons. However, such binders rely on a single type of solvent water, and cannot be stably dispersed in an aqueous solution for a long time, and the slurry is prone to sedimentation, so that various components in the electrode are unevenly distributed, and efficient electron and ion transmission in the electrode cannot be guaranteed.
Therefore, the current breakthrough point of industrialization of the aqueous binder for the lithium ion battery cathode material is to develop a binder with excellent dispersibility, film-forming property and chemical stability: the binder is required to be stably dispersed in an aqueous solution for a long time, does not settle and exist stably, is not limited to a single solvent, has excellent electronic conductivity and ionic conductivity, can solve the problem of dispersibility of the binder and conductive particles in the preparation process of electrode slurry, realizes uniform distribution of various components in an electrode, and can ensure efficient electronic and ionic transmission in the electrode.
Disclosure of Invention
The invention provides a composite binder applied to a lithium ion battery anode material aiming at the problems, which is characterized in that the binder is compounded by an ionic polymer, an electronic conducting polymer and an adhesive, wherein the ionic polymer, the electronic conducting polymer and the adhesive are used for preparing the composite binder, and the composite binder is prepared by mixing the ionic polymer, the electronic conducting polymer and the adhesive
The ionic polymer is selected from one or more of lithium polyacrylate and derivatives thereof;
the electron conductive polymer is selected from one or more of poly 3, 4-ethylenedioxythiophene/polystyrene sulfonate and derivatives thereof;
the adhesive is selected from one or more of polyacrylic acid, polyacrylic acid derivatives, polyvinylpyrrolidone and polyvinylpyrrolidone derivatives.
The composite binder does not contain solvent, wherein the ionic polymer accounts for 10-80 wt% of the composite binder, the electronic conductive polymer accounts for 10-40 wt% of the composite binder, and the adhesive accounts for 1-80 wt% of the composite binder.
More preferably, the ionic polymer accounts for 40-45% of the composite binder by weight.
More preferably, the electronic conducting polymer accounts for 10-20% of the composite binder by weight.
More preferably, the adhesive accounts for 40-45% of the composite binder by weight.
Among them, preferred components are as follows:
the adhesive disclosed by the invention can solve the problem that the adhesive can be dissolved only by heating in the industry, so that the novel adhesive has room-temperature solubility, and the adhesive can be dissolved by using an aqueous solvent or a non-aqueous solvent, thereby reducing the pollution problem to the environment and meeting the requirements of industrial production. The composite adhesive has ionic conductivity and electronic conductivity, meets the physical properties of a pole piece, and forms an ionic/electronic conductive network to enhance the electrochemical performance of the battery.
The invention also aims to provide a preparation method of the composite binder applied to the lithium ion battery anode material, which comprises the following preparation steps:
(1) preparation of ionic polymer solution: reacting a polymer containing-COOH groups with LiOH, freezing and drying to obtain an ionic polymer, and dissolving the ionic polymer in a solvent to form an ionic polymer solution;
(2) preparing a binder solution: adding the electron conductive polymer dispersion liquid in the step (1), mixing at room temperature to form a mixed liquid, and standing. And blending the mixed solution with an adhesive to obtain a ternary compound solution.
(3) Preparation of a composite film: and (3) dripping the ternary compound solution onto a clean glass sheet at room temperature, coating to form a film, and removing the solvent to obtain the composite film.
The purpose of the preparation of the composite film is that the adhesive mainly acts between the active material and the conductive particles in the form of a film, so that experimental research is designed to test various properties of the composite film so as to judge whether the prepared composite meets the basic conditions of the lithium ion battery adhesive.
Wherein the solvent is one or more of deionized water, acetonitrile, ethanol, methanol, isopropanol, glycol, glycerol, dimethyl sulfoxide, dimethylformamide, dimethyl sulfone, tetrahydrofuran and N-methylpyrrolidone.
Preferably, the solvent is deionized water or N-methyl pyrrolidone.
The composite binder can be dissolved by an aqueous solvent or a non-aqueous solvent, and because a plurality of hydrophilic functional groups are arranged in the side chain of the composition for forming the composite binder, the composite binder can generate stronger hydrogen bonds with an active substance and a current collector, and provides better adhesion performance.
In the above preparation steps, the method for preparing lithium polyacrylate of step (1): weighing a certain amount of polymer polyacrylic acid, adding a 5% lithium salt aqueous solution by mass, stirring to obtain a mixed solution, freeze-drying to obtain lithium polyacrylate powder, and sealing and storing in a dryer for later use. Weighing a certain amount of lithium polyacrylate in a beaker, adding distilled water or NMP, stirring at room temperature until the lithium polyacrylate is completely dissolved to form ionic polymer water/NMP solution with a certain mass fraction,
step (2) preparation method of binder solution: adding a certain amount of PEDOT: PSS dispersion liquid in the step (1), placing the mixture at room temperature, magnetically stirring the mixture for 5 hours to ensure that the mixture is completely mixed to form a lithium polyacrylate PAALi/PEDOT: PSS mixed solution, and standing the mixture for 24 hours. Respectively blending the mixed solution with PVP polyvinylpyrrolidone and PAA polyacrylic acid, stirring at room temperature until the mixed solution is uniformly mixed to obtain two ternary compound solutions of PAALi/PEDOT, PSS/PAA and PAALi/PEDOT, PSS/PVP, and respectively abbreviated as PAALi/PEDOT, PSS/PAA/H and the product of the two ternary compounds after being dissolved in solvent water or NMP2O, PAALi/PEDOT PSS/PAA/NMP and PAALi/PEDOT PSS/PVP/H2O、PAALi/PEDOT:PSS/PVP/NMP。
The preparation method of the compound film in the step (3) comprises the following steps: dripping the polymer mixed solution on a clean glass sheet at room temperature, coating the glass sheet with a scraper to form the same thickness, placing the glass sheet in a constant-temperature drying oven at 70 ℃ to remove the solvent, repeating the steps for a plurality of times to enable the film to reach a certain thickness, and transferring the film to a vacuum drying oven at 80 ℃ to be dried in vacuum for 12 hours to obtain the composite film.
Compared with the prior art, the composite binder can be dissolved in a water solvent or a non-water solvent, adopts the most basic lithium battery binder material in the preparation process, has rich sources, simple preparation process, no need of adding a stabilizer, suitability for industrial production and excellent electrochemical performance.
Drawings
FIG. 1 is a flow chart of a process for preparing a lithium ion battery by using a water/water-insoluble composite binder.
FIG. 2 use of PVDF as a binder with LiFePO prepared using a composite binder4Graph comparing rate performance of half cell at room temperature.
FIG. 3 PVDF-based LiFePO4Half cell and composite binder based LiFePO4Graph comparing the cycling performance of half cells at different temperatures.
Detailed Description
The present invention will be described in further detail below with reference to specific embodiments and accompanying drawings. The following examples are not intended to limit the scope of the present invention.
In the experiment, the positive plate prepared by the composite binder is further assembled into a battery, and the application effect of the invention is demonstrated by testing and inspecting the coating performance of the positive plate, the electrochemical performance of the battery and the like.
Material sources are as follows: all materials were purchased commercially unless otherwise specified.
Application of the composite binder of the present invention to electrode fabrication and battery assembly was prepared by the method shown in fig. 1, wherein the abbreviation PA-L stands for PAALi; PV/PA stands for PVP/PAA; PT stands for PEDOT: PSS:
example 1 an aqueous dispersion of an ionic polymer solution PAALi and an aqueous dispersion of an electronic conductive polymer PEDOT: PSS were magnetically stirred for 5 hours at room temperature using water as a solvent to be completely mixed to form an aqueous solution mixture of PAALi/PEDOT: PSS, followed by addition of a binder PVP, and uniformly stirred to form an aqueous composite binder of PAALi/PEDOT: PSS/PVP, respectively. With LiFePO4And (3) preparing a positive plate from the positive material, wherein the positive plate comprises the following components: 80 parts of positive electrode material, 10 parts of acetylene black, 10 parts of composite binder and 100 parts of solvent. Then sequentially adding acetylene black and active substances and stirring to prepare slurry; after materials are uniformly mixed, coating the slurry on an aluminum foil by a scraper with a certain thickness, drying the aluminum foil for 2.5 hours in an electric heating constant-temperature air-blast drying oven at the temperature of 60 ℃ to obtain an anode plate with the thickness of about 30 mu m, cutting the anode plate into round thin sheets, transferring the round thin sheets into a vacuum drying oven for drying for 12 hours, cooling, weighing the mass of an electrode plate, and putting the electrode plate into a glove box. And placing the gasket, the lithium sheet, the diaphragm and the positive plate in a glove box in a high-purity argon atmosphere from bottom to top in sequence into a negative electrode shell, dropwise adding electrolyte, tightly covering the positive electrode shell, and sealing and packaging to obtain the R2016 type button lithium ion battery for testing.
The addition of the composite binder component calculated according to the percentage is shown in the following table 1, the physical performance test is carried out on the anode pole piece prepared under the condition, and the anode pole piece is assembled into a button type lithium ion half cell for carrying out the electrochemical performance test.
TABLE 1PAALi/PEDOT PSS/PVP/H2Factor level meter for O composite binder
Example 2 the procedure is as above, except that the adhesive is PAA and the amount of the composite binder component added in percent is as shown in table 2 below:
TABLE 2PAALi/PEDOT PSS/PAA/H2Factor level meter for O composite binder
Example 3 the process steps are as above except that the solvent is NMP and the adhesive is PVP, and the amounts of the components of the composite binder added, calculated as percentages, are as follows in table 3:
TABLE 3PAALi/PEDOT PSS/PVP/NMP composite Binder factor level Table
Example 4 the procedure is as above, except that the solvent is NMP and the adhesive is PAA, and the amounts of the components of the composite binder added in percent are as shown in table 4 below:
TABLE 4PAALi/PEDOT PSS/PAA/NMP composite Binder factor level Table
Note: the addition amount of the composite binder in tables 1 to 4 is calculated according to the addition amount of 0.1g of PVDF in the control group, wherein the ratio of the binder to the conductive agent to the active material is 10: 10: 80.
example 5 the method steps are as above, except that the ratio of binder, conductive agent, active substance is 8: 12: 80, the percentage of each component in the adhesive in the composite adhesive is respectively as follows: PAALi 42%, PVP 42%, PEDOT PSS 16%.
Example 6 the method steps are as above, except that the ratio of binder, conductive agent, active substance is 12: 8: 80, the percentage of each component in the adhesive in the composite adhesive is respectively as follows: PAALi 42%, PVP 42%, PEDOT PSS 16%.
Example 7 the procedure was as above, except that the active material was changed to LiNi1/3Co1/3Mn1/3O2The proportion of the binder, the conductive agent and the active substance is 10: 10: 80.
(1) preparation of positive plate
Coating the slurry prepared by the above by a scraper, taking a single-sided aluminum foil with the thickness of 20um as a current collector, and naturally airing to obtain the positive plate, wherein the coating thickness is 400 um.
(2) Coating performance test of positive plate
After being dried, the positive plate is tested for adhesion and flexibility according to national standards GB/T9286-1998 and GB/T1731-1993 respectively.
(3) Battery assembly
Cutting the dried positive plate into small round plates with the diameter of 14mm, placing the small round plates in an oven at 80 ℃, baking for 8h, drying at 120 ℃ in vacuum for 12h, weighing, assembling a button cell by taking a lithium plate as a negative plate in a glove box, sealing, and carrying out electrical property test.
(4) Battery testing
And placing the sealed battery on a LAND blue test system, standing for 3h, charging to the required voltage, then charging at constant voltage for 0.5h, and finally discharging to the required voltage at the required multiplying power.
Comparative example: respectively with LiFePO4、LiNi1/3Co1/3Mn1/3O2The positive plate is prepared by taking a positive electrode material, polyvinylidene fluoride (PVDF) as a binder and N-methyl pyrrolidone (NMP) as a solvent, and the positive electrode plate comprises the following components: 80 parts of positive electrode material, 10 parts of acetylene black, 10 parts of PVDF and 100 parts of NMP. According to the stepsThe battery is prepared, and the difference is that when PVDF is dissolved in NMP, the temperature is required to be heated to 45 ℃, and the heating time is 3-5 h; and directly placing the slurry in an oven for drying after coating. And (3) carrying out physical performance test on the positive pole piece prepared under the condition, and assembling the positive pole piece into a button type lithium ion half cell to carry out electrochemical performance test.
Tests show that LiFePO prepared by the composite binder of the invention4The film forming of the positive plate is good, the positive plate has no crack, and the flexibility and the adhesive force of the positive plate are qualified; the absorption capacity of the composite binder to the electrolyte is greater than that of a PVDF binder, and the internal structure is not damaged due to the swelling phenomenon, so that the lithium ion transmission in the pole piece can be met; the composite binder enables LiFePO to be used4And the conductive particles are uniformly dispersed to form a good conductive network, and the occurrence of agglomeration is reduced. LiFePO prepared by using composite binder of the invention4The half cell has good normal temperature rate performance, cycle performance and high temperature (55 ℃) cycle performance, and the discharge specific capacity is 40.25mAh g under high rate (20℃)-1Much higher than 13.12mAh g of PVDF binder battery-1At high temperature (55 ℃), the capacity retention rate of 99.94 percent is still remained after 100 cycles, which is slightly higher than that of PVDF/LiFePO4Half cell (98.95%).
The test results are shown in tables 1 to 2 and FIGS. 1 to 2.
TABLE 1 LiFePO of PVDF with composite Binder (PAALi/PEDOT: PSS/PVP)4Comparison of electrolyte absorption of Positive electrode sheet
TABLE 2 results of flexibility and adhesion tests
Note: the addition amount of the composite binder is calculated according to the addition amount of 0.1g of PVDF in a control group, wherein the ratio of the binder to the conductive agent to the active substance is 10: 10: 80.
Claims (8)
1. a composite binder applied to a lithium ion battery anode material is characterized in that the binder consists of an ionic polymer, an electronic conducting polymer and an adhesive; wherein the content of the first and second substances,
the ionic polymer is lithium polyacrylate;
the electron conducting polymer is poly 3, 4-ethylenedioxythiophene/polystyrene sulfonate;
the adhesive is selected from polyacrylic acid or polyvinylpyrrolidone;
the composite binder does not contain a solvent, and the ionic polymer, the electronic conducting polymer and the adhesive respectively account for 10-80%, 10-40% and 1-80% of the composite binder by weight percent.
2. The composite binder of claim 1, wherein: the ionic polymer accounts for 40-45% of the composite binder by weight.
3. The composite binder of claim 1, wherein: the weight percentage of the electronic conductive polymer in the composite binder is 10-20%.
4. The composite binder of claim 1, wherein: the adhesive accounts for 40 to 45 percent of the weight of the composite binder.
5. A preparation method of a composite binder applied to a lithium ion battery anode material is characterized by comprising the following preparation steps:
(1) preparation of ionic polymer solution: reacting a polymer containing-COOH groups with LiOH, freezing and drying to obtain an ionic polymer, and dissolving the ionic polymer in a solvent to form an ionic polymer solution;
(2) preparing a binder solution: adding the electron conductive polymer dispersion liquid in the step (1), mixing at room temperature to form a mixed liquid, standing, and blending the mixed liquid and an adhesive to obtain a ternary compound solution;
(3) preparation of a composite film: dripping the ternary complex solution on a clean glass sheet at room temperature, coating to form a film, and removing the solvent to obtain a composite film;
wherein: the solvent in the step (1) is one or more selected from deionized water, acetonitrile, ethanol, methanol, isopropanol, glycol, glycerol, dimethyl sulfoxide, dimethylformamide, dimethyl sulfone, tetrahydrofuran and N-methylpyrrolidone;
the ionic polymer is lithium polyacrylate; the electron conducting polymer is poly 3, 4-ethylenedioxythiophene/polystyrene sulfonate; the adhesive is polyacrylic acid or polyvinylpyrrolidone; the ionic polymer, the electronic conducting polymer and the adhesive respectively account for 10-80 percent, 10-40 percent and 1-80 percent of the composite binder by weight percent;
the composite binder prepared by the method is dissolved in an aqueous solvent or a non-aqueous solvent at room temperature.
6. The production method according to claim 5, wherein the solvent in step (1) is water or N-methylpyrrolidone.
7. A preparation method of a positive plate of a lithium ion battery is characterized by comprising the following steps: the composite binder according to any one of claims 1 to 4 is used in the production process of the positive electrode sheet.
8. A lithium ion battery, characterized in that the binder material of the positive electrode sheet of the lithium ion battery contains the composite binder according to any one of claims 1 to 4.
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| CN111253534A (en) * | 2019-12-30 | 2020-06-09 | 深圳市研一新材料有限责任公司 | Preparation method of aqueous lithium supplement binder and positive plate for lithium ion battery |
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| CN114361456B (en) * | 2022-01-11 | 2023-05-05 | 中国科学院化学研究所 | Water-based functional ion-conducting binder for lithium battery, preparation method and application |
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| CN114805823A (en) * | 2022-04-25 | 2022-07-29 | 惠州锂威新能源科技有限公司 | Crosslinked composite binder, preparation method thereof, pole piece and secondary battery |
| CN115425226B (en) * | 2022-08-18 | 2023-04-14 | 楚能新能源股份有限公司 | Ternary material flexible positive electrode and preparation method thereof |
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| "PAA/PEDOT:PSS as a multifunctional, water-soluble binder to improve the capacity and stability of lithium-sulfur batteries";J.Pan;《RSC Advances》;20160413;第1-6页 * |
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| Publication number | Publication date |
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| CN109167064A (en) | 2019-01-08 |
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